Method of producing a viscous phenol condensation product



Patented Apr. 30, 1929.

UNITED STATES PATENT oFFlcE.

RICHARD G'U'NTZEL, OF SAAIiFELD-SAALE, GERMANY, ASSIGNOR TO TH E FIRMSCHIE- FERWERKE AUSDAUEB AKTIENGESELLSGHAFT, OF PROBSTZELLA, THURINGIA,I

GERMANY.

METHOD OF PRODUCING A VISCOTJ'S PHEIN'OL CONDENSA'DION -PRODUC'1.

1\To Drawing. Application filed March 8, 1928, Serial No. 260,258, andin Germany Iviarch 10, 1927.

5 es s with subsequent hardening. Initial materials for the newcondensation product are formaldehyde, commercial phenol andp-dichlorobenzen'e. As condensation catalyst, use is made of a mixedsalt consisting of hexamethylene tetramine,sodium chloride and am- Imonium chloride, which is prepared by introducing formaldehyde orformalineinto an aqueous solution of ammonium chloride, which. issupersaturated with sodium bicarbonate. It has been found that this saltmixture is an excellent catalyst.

The condensation product can according to the following example:

1 lit. of the usual crystallized commercial phenol is liquefied byheating and mixed with about 600 ccms. 40% formaldehyde solution. Aquantity of p-dichlorobenzene corresponding to about 8% p 7 the phenolused is then added, heating being continued until this substance is alsoliquefied. If the whole is vigorously stirred, it dissolves to form ahomogeneous mixture. To, this mass is then added a mixed salt,consisting of about parts'common salt, 10 parts ammonium chloride and30parts hexamethyl.

' ene tetramine, in a quantity corresponding to about 1% of the amountby weight of the phenol used. The whole is now heated to boiling, usinga reflux condenser. A condensation product is formed, which soonseparates from the water. The heating is now discontinued, and afterwaiting for a time until the reaction is complete, the water is drawn01f. Evaporation is carried out for a time and then cold water poured in*while stirring. A further vigorous reaction takes place and the partscoming to the surface upon stirring, decompose showing a colourphenomenon (rainbow colours). This reaction is assisted by breaking upthe clear film of resin which is formed and bringing other parts to thetop until the reaction has ceased. The water is then re- I newed, untilafter changing the water several times, no-further reaction occurs. Thewater is now removed by decanting with subsequent be prepared of theamount by weight of V evaporation of the last traces. A liquid productof syrup-like consistency and light in colour is obtained. The mass isnow ready to be used for the purpose in View. By hardening it can beconverted in a known manner into solid bodies. The hardened'products areof light to dark-yellow colour, transparent to translucent and areelectrified by friction like amber.

The non-hardened, viscous mass has the advantage over other condensationproducts that it can be converted into a hard, solid mass in a veryshort time, by being only slightly heated to about C. A subsequentslight heating of comparatively short duration is then suflicient toimpart to the substances prepared from the mass, a degree of hardnesswhich in the case of other known condensation products heated to thesame or greater ex"- weeks.

WVhat Iclaim is 1. A method of producing a viscous condensat-ionproduct, consisting in heating to boiling point a mixture of phenol,p-dichlorobenzene and formaldehyde in the presence of 'a mixed saltconsisting of common salt, ammonium chloride and hexamethylene tetranine, eliminating the water which separates but driving oil volatilevapors, washing carefully with water and thereupon hardening as and forthe purpose set forth.

2. A method of producing a viscous condensation product, consistingin'heating to boiling point a mixture composed of about 8% by weight ofp-dichlorobenzene to each litre of crystallized commercial phenol andabout 600 ccms. of a 40% formaldehyde solution, in the presence of aquantity corresponding to about 1% of the welght of the phenol, of amixed salt composed of about 60 parts common salt,

10 parts '-ammonium chloride and 30 parts hexamethylene tetramin'e,eliminating the water which'separates out, driving-oft volatile vapors,washingearefully with water and thereupon hardening as and for thepurpose set forth.

Intestimony whereof I hereunto aflix my signature.

. menial) euNTzEL.

